Apparatus for recovering spent adsorbent material



Feb. 22, 1944. FAST 2,342,622

APPARATUS FOR RECOVERING SPENT ,ADSORBENT MATERIAL Original Filed Oct. l, 1938 Jeam eweraar pregare faire (v0 [tifa/(afar f a Kompressor MQW.

ATTORNEY Patented Feb. 22, 1944 APPARATUS FOR RECOVERING SPENT ADSOBBENT MATERIAL Fred L. Fast, Woodbury, N. J., assignor to Soco'ny- Vacuum Oil Company, Incorporated, New York. N. Y.. a corporation of New York ylriginal application'october 1, 1938, Serial No.

Divided and this application December 19, 1940, Serial N0. 370,753

Claims. Cl. 2oz-421) Numerous processes, such as the percolation filtration of mineral petroleum oils; clarification of oils, fats, sugar, etc., by nltration; and similar processes, result in contamination of the adsorbent mass used by combustible carbonaceous material. Similarly many catalytic processes using as a catalyst an adsorbent or refractory contact mass which is catalytic in nature orhas a catalyst material supported upon it or impregnated in it also contaminate the contact mass with a combustible carbonaceous material. It is customary to regenerate such adsorbents and contact masses by burning on the contaminant. This invention is specifically concerned with such processes of regeneration.

Such processes must operate within narrowly deilned limits of temperature. The temperature must be su'lciently high to enable combustion to take place, yet it must not be too high, for practically all of the adsorbents so used may be permanently damaged by temperatures readily reached. As an illustrative example, without being limited thereto, the regeneration of spent iullers earth from a process of petroleum retinving may be considered. This material may be ldamaged seriously by exposure to temperatures above about 1100l200 F. for any length of time.

Yet it must be heated to at least about 800850 F., and preferably between about'850 vand about 1050 F., to undergo combustion, and the combustion is highlyv exothermic when the carbonaceous material is burned with air asis conventional. Consequently, such regenerations are dilcult to control. y

This invention has for aprincipal object the provision of an apparatus for the regeneration or spent adsorbent material wherein the material undergoing `regeneration is subjected to an endothermic regeneration reaction in a cyclic process wherein an exothermic reaction is separately conducted, the endothermic reaction and the exothermic reaction being conducted in paress. wherein I is a chamber containing spent adsorbent to be regenerated, and 2 is a pipe through which compressed gas is led thereinto. Pipe 3 depends toward the bottom of I and when valve 4 is opened, adsorbent will pass upward through 3, I, tubes 5 in preheater 6, and then through the annular passage within r'1, where it is regenerated by a reaction hereinafter explained. Passing from regenerator 'I through gooseneck 8 to collector 9, the regenerated adsorbent is separated from the gases accompanying it and removed from the system by pipe I0.

Regeneration medium -introduced by pipe II is carbon dioxide gas, or carbon dioxide gas adlmixed with nitrogen or air, in such ratios of mixture that any reaction between the regeneration medium and the carbonaceous deposit upon the spent adsorbent is an endothermic reaction, such as the reaction which predominates.

The effluent gases from regeneration, rich in carbon monoxide, pass from collector .9 into pipe I2, whence a portion of these gases are lead through pipe I3 by gas pump I4, and introduced through pipe I5 into combustion tube I6, which is centrally disposed in regenerator 1. Air for the exothermic combustion of carbon monoxide to carbon dioxideis provided from pipe I'I through a plurality of spaced inlets I8. The exothermic combustion occurring within tube I6 is controlled to furnish a proper amount of heat for the endothermic regeneration occurring` in regenerator 'I surrounding tube I8. A portion ot the carbon monoxide-containing gas is diverted from pipe I5 by pipe I9 and led to burner 20, wherein it is burned to furnish heat for preheater 6, the flue gases from which are exhausted to atmosphere through vent 2 I.

A further portion of the gases from regenera tion, rich in carbon monoxide, are led by pipe 22 to combustion chamber 23, to which air is introduced from pipe I1 by pipe 24. Within chamber 23, these gases are subjected to exothermic combustion to carbon dioxide. oxide-containing gases from combustion tube I6 -are led into chamber 23 byv pipe 25. -v

pipe 21, from whicha portion passes through pipe The carbon di- 28 and gas pump 2l to pipe Il to be introduced to the regeneration as a source ofcarbon dioxide. Pipe 30, connecting pipes 28 and 22 is for use in starting up during the period prior to the establishment o! normal operating atmospheres within the various portions of the system. A portion of the partially cooled gases from pipe 2l are passed through a waste heat boiler 3| and exhausted to atmosphere through vent valve 32. A portion of the gas from pipe 28, after passing through feed water heater 3l wherein it is cooled, is compressed by compressor 34 and passed .through pipe 2 to vessel I to furnish the motive power to introduce spent adsorbent therefrom into the system. If desired, steam maybe admitted to the regeneration reaction either at the regenerator by valve II or before preheat by valve 36. This steam may be superheated, -if desired, by passage through the preheater in pipe 31, as shown. y

It will be observed that'the principle of operation followed herein is that of a wholly endothermic regeneration reaction conducted in heat exchange relationship'with an exothermic combustion of regeneration products and controlled by the conduct of such exothermic reaction. The control is achieved by varying the intensity of the burning of carbon monoxide in pipe I8, as by varying the amountof gas introduced by pump I4 and air introduced by pipe I8.

It is to be preferred, that the adsorbent to be regenerated 'should be at least partially freed of those contaminants which can be removed by physical means. For example, fullers earth used in petroleum illtration should be steamed until substantially i'ree of entrained oil or wash liquor prior to being charged to the system herein set forth.

As indicated above, the regeneration medium,

need not be entirely oxygen-free. In fact, it is likely that it will not be solely a mixture of carbon 'dioxide and nitrogen such as'would result from complete consumption of air. It will normally contain, in addition to these, some carbon monoxide, some water vapor and some oxygen. Itis important, though, that the relative per- `centages of these materials should be suiiiciently low so that the regeneration reaction is substantially endothermicin nature, resulting in the production of a subnantial relative proportion of carbon monoxide.

y It is recognized that there are known processes of regeneration wherein the spent adsorbent is regenerated in an atmosphere which may be diluted by the `return thereto of ilue gas produced by the regeneration, which flue gas containscarbon dioxide, the dilution probably resulting in some incomplete 4combustion with resulting production of carbon monoxide. This process does vnot partake of that nature being conducted with a regenerating medium suiiiciently devoid of free oxygen, and sumciently rich in carbon dioxide, for the predominant Vreaction to be the endov`thermic reaction between carbon and carbon dioxide to form carbon monoxide. It is also recognized that there areknown processes wherein the spent adsorbent is regenerated in an isolated atmosphere, (which may be reducing) in a passage surrounded by a combustion to which ilue gas from said combustion has been returned to control its intensity. It will be recognized that this principle is not made use of here.

It win further be recognized, S0 far as apparatus is concerned. that many other forms of apparatus may be provided in which the process may be carried out. yet that all these are a part for introducing spent adsorbents to said regenerof my invention, subject to limitations as claimed. For example, since the heat demand for the endothermic reaction CO2+C 2CO for one pound of carbon contaminant is less than the corresponding heat available from the reaction 2CO+O2 2CO2, there are provided two combustion zones, viz, I6 and 23. It will be obvious that either a portion oi.' the gases may be burned in I6, or that all may be burned in 23 and a portion led in heat, exchange with 1 to provide needed heat, or all may be burned in 23 and some iiuid heat transfer medium may be used to transfer heat from 23 to 1.

,While it is preferable to conduct` the operation shown under pressure slightly above atmospheric to prevent infiltration of unwanted air, 'the pressure may be increased considerably above this, if desired, to secure more rapid and more thorough reaction.

This application is a division of my co-pending d application S. N; 232,745, filed October 1, 1938, now United States Patent #2,261,151.

I claim:

l. An apparatus for regenerating spent adsorbents carrying carbonaceous impurities com'- prising an elongated regenerating chamber, means for introducing-spent adsorbents to said chamber and means for removing regenerated adsorbents from the opposite end thereof, means for introducing a gaseous regenerating agent to said chamber and means at the opposite end thereof for withdrawing ue gases, a separate combustion chamber equipped to convert carbon monoxide to carbon dioxide and positioned in indirect heat exchange With said regenerating chamber, means for introducing gas to said combustio'n chamber and means at the opposite end thereof for withdrawing ilue gases, a gas line for ities comprising two elongated, concentric cham-v bers which are separated by a heat conducting wall so that the chambers are in indirect heat exchange with each other, means for admitting spent adsorbents to one of said chambers and -means forwithdrawing regenerated adsorbents from the opposite end thereof, means for introducing a gaseous regenerating agent to this ilrst chamber and means at the opposite end thereof for withdrawing flue gases, means for introducing gas to the second chamber ,and means at the opposite end thereof for removing ue gases, a. gas line for passing ue gases withdrawn from said first chamber to said means for introducing gas to said second chamber, and a gas line for passing flue gases withdrawn from said second chamber to said means for introducing gas to said first chamber.

3. Anapparatus for regenerating spent adsorbent particles carrying carbonaceous impurities comprising an elongated regenerating cham-f ber adjoining to and in indirect heat exchange relationship with a iirst combustion chamber, a second independent combustion chamber, means for introducing gas to and withdrawing ilue gas from each of said combustion chambers, means ating chamber and means for removing regenerated adsorbents from the opposite end thereof,

means for introducing a gaseous -regenerating agent to said regenerating chamber and means at the opposite end thereof for withdrawing ilue gases, gas line means for passing flue gas withdrawn from said regenerating chamber to each of said combustion chambers, and gas line means for passing ilue gases withdrawn from each of said combustion chambers to said regenerating chamber.

4. An apparatus for regenerating spent noncarbonaceous contact material carrying carbonaceous impurities comprising an elongated regenerating chamber, means for suspending said spent contact material in a stream of gaseous regenerating agent, means for introducing said stream oi' gaseous regenerating agent carryingsaid spent contact material into said elongated chamber, means at the opposite end of said chamv ber for withdrawing gaseous agent carrying suspended contact material, means for separating suspended contact material from said withdrawn gaseous agent, a separate combustion chamber equipped to convert carbon monoxide t'o carbon dioxide and positioned in indirect heat exchange.

relationship with said regeneratingv chamber, means for introducing gas to said combustion chamber and means at the opposite end thereof for-removing gas.4 a gas line for passing said gaseous agent from said contact materialseparating means to said means for introducing gas to said combustion chamber, and a gas line for passing gases removed from said combustion chamber to said regenerating chamber. i 5. Apparatus for regenerating spent non-carbonaceous `contact material carrying carbonaceous impurities which comprises, a vertically elongated regenerating chamber, a plurality of conduits discharging into the bottom. of said' chamber' in substantially parallel relationship 'along the long axis thereof, feed chamber means i'or spent contact material disposed below said regenerating chamber, passageway defining means leading upwardly from vsaid feed chamber means to said conduits, means for passing regenerating gas upwardly through said passageway detlning means so as to carry spent contact material in suspension iromsaid feed chamber means through said conduits into and through said regenerating l chamber, a solid gas separatordisposed in the 

